CN106571172A - Aluminum alloy substrate thick film circuit intermediate-temperature sintering dielectric paste and preparation method thereof - Google Patents

Aluminum alloy substrate thick film circuit intermediate-temperature sintering dielectric paste and preparation method thereof Download PDF

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Publication number
CN106571172A
CN106571172A CN201610853299.4A CN201610853299A CN106571172A CN 106571172 A CN106571172 A CN 106571172A CN 201610853299 A CN201610853299 A CN 201610853299A CN 106571172 A CN106571172 A CN 106571172A
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thick film
dielectric paste
film circuit
aluminium alloy
base plate
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高丽萍
苏冠贤
张念柏
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Dongguan Corehelm Electronic Material Technology Co Ltd
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Dongguan Corehelm Electronic Material Technology Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/002—Inhomogeneous material in general
    • H01B3/006—Other inhomogeneous material
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C12/00—Powdered glass; Bead compositions
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
    • H01B3/00—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties
    • H01B3/02—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances
    • H01B3/08—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of inorganic substances quartz; glass; glass wool; slag wool; vitreous enamels
    • H01B3/087—Chemical composition of glass

Abstract

The invention discloses an aluminum alloy substrate thick film circuit middle-temperature sintering dielectric paste and a preparation method thereof. The preparation method is used for preparing the aluminum alloy substrate thick film circuit middle-temperature sintering dielectric paste. The aluminum alloy substrate thick film circuit middle-temperature sintering dielectric paste comprises the following materials in part by weight: 60%-80% of lead-free microcrystalline glass powders, 1%-10% of rare earth oxide and 19%-30% of organic bonding phase, wherein the lead-free microcrystalline glass powders are formed by SiO2, Bi2O3, B2O3, ZnO, K2O, SrO2 and CaO; and the organic bonding phase is a mixture formed by an organic solvent, a high-polymer thickener, a surfactant, a plasticizer, a dispersant, an antifoaming agent and a thixotropic agent. A dielectric layer formed by printing the dielectric paste on an aluminum alloy substrate has the advantages of large adhesive force, large breakdown strength and high insulation resistance, and is capable of being compatible with a thick film circuit of the aluminum alloy substrate with a resistance paste and an electrode paste.

Description

A kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste and preparation method thereof
Technical field
The present invention relates to thick film circuit technique field, more particularly to a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature medium Slurry and preparation method thereof.
Background technology
As thick film circuit element is to multiple stratification and the development of miniaturization, corresponding mechanics and thermal property are proposed to substrate Require, particularly the thermal conductivity of substrate is required.It is cold that density that aluminium alloy base plate has is little, ductility is good, thermal conductivity is good, excellent The performance such as thermo forming performance and good toughness makes it possible to be used as baseplate material, but thus brings again The problems such as mismatch of thermal coefficient of expansion and conventional electric slurry.
Aluminium alloy proposes to be different from general dielectric paste as baseplate material to the dielectric paste for preparing thick film integrated circuit Technical requirements, specially：1st, processing performance：Due to the fusion temperature of aluminium alloy it is relatively low（660 DEG C or so）, it is impossible to select high temperature Standard firing process（850℃）, it requires that corresponding dielectric paste can only be sintered under the fusion temperature less than aluminium, and have good Good adhesive force, matching, in addition to meet element electrical performance demands, need on substrate multiple serigraphy, dry, burn till Deng to obtain adequate thickness, increasingly complex technical requirements, including screen printing property and multiple reheating are thus proposed to slurry Property（550℃）；2nd, physical property：Dielectric paste aluminium alloy plate surface by silk-screen, the technique such as burn till and obtain insulating barrier, it is preferable The acquisition of insulating barrier is obviously relevant with the function phase related physical performance of dielectric paste, and these performances include expansion character, heat conduction The bonding force of performance, heat resistance and aluminium alloy base plate；3rd, electric property：As between aluminium alloy and resistance track and electrode Insulating barrier, dielectric paste organizine print burn till after should possess good electric property, including breakdown strength, insulaion resistance, leakage Electric current；4th, environmental requirement：When thick film circuit is used as electronic component, should also there is the requirement without noxious material, to corresponding Electric slurry is just free from the heavy metal such as element such as cadmium, lead, mercury.
At present, the dielectric paste of thick film circuit on the market based on stainless steel substrate ripe and commercialization, but be applied to The dielectric paste of aluminium alloy base plate is less；Patent No. 200910310045.8, patent name is for " a kind of metal aluminum substrate is thick The Chinese invention patent and Application No. 201510334158.7, patent of dielectric paste of film circuit and preparation method thereof " The Chinese invention patent of entitled " one kind is for aluminium base thick film circuit dielectric slurry and preparation method thereof " is disclosed respectively For aluminium base thick film circuit dielectric slurry and preparation method thereof, but the sintering temperature of these Alumina-Based Media slurries is inclined Height, while breakdown voltage and insulaion resistance can not still meet the high request of aluminium base heating.
The content of the invention
Present invention aims to the deficiencies in the prior art and a kind of middle temperature of aluminium alloy base plate thick film circuit is provided and is burnt Knot dielectric paste, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste can match well with aluminium alloy base plate, Breakdown strength is big, insulaion resistance is high, can be compatible with the thick film circuit resistance slurry of aluminium alloy base plate and electrode slurry.
Another object of the present invention is to provide a kind of preparation of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste Method, the preparation method can effectively be produced and prepare above-mentioned dielectric paste.
For achieving the above object, the present invention is achieved through the following technical solutions.
A kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, includes the material of following weight portion, specially：
Leadless crystallizing glass powder 60% ~ 80%
Rare earth oxide 1% ~ 10%
Organic bonding phase 19% ~ 30%；
Wherein, leadless crystallizing glass powder is by SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, seven kinds of materials of CaO composition, it is unleaded micro- SiO in crystal glass powder2、Bi2O3、B2O3、ZnO、K2O、SrO2, seven kinds of materials of CaO weight portion be followed successively by 20% ~ 30%, 10% ~ 20%、10%~20%、10%~20%、10%~20%、5%~10%、5%~10%；
Organic bonding is mutually organic solvent, macromolecule thickener, surfactant, plasticizer, dispersant, defoamer, thixotropic agent The mixture that seven kinds of materials are constituted, organic solvent in organic bonding phase, macromolecule thickener, surfactant, plasticizer, point Powder, defoamer, the weight portion of eight kinds of materials of thixotropic agent be followed successively by 30% ~ 60%, 20% ~ 30%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%、1%~5%。
Wherein, the particle size values of the leadless crystallizing glass powder are 1 ~ 3 μm, and softening point is 350 ~ 450 DEG C, average line expansion system Number is 18 ~ 25 × 10-6/℃。
Wherein, the rare earth oxide is La2O3、Sc2O3、Y2O3、CeO2、Sm2O3、Gd2O3、Nd2O3、Pr2O3、Eu2O3In One kind, the particle size values of rare earth oxide are 1 ~ 3 μm.
Wherein, the organic solvent be turpentine oil, terpinol, hexadecanol, butyl carbitol, butyl carbitol acetate, Diethylene glycol monomethyl ether, dibutyl ethylene glycol ether, ethylene glycol ether acetate, ATBC, tributyl phosphate, Isosorbide-5-Nitrae-fourth In lactone, mixed dibasic acid ester, 1-METHYLPYRROLIDONE, DMF, DMA, dimethyl sulfoxide A kind of or at least two mixtures for being constituted.
Wherein, the macromolecule thickener is ethyl cellulose, hydroxyethyl cellulose, carboxymethylcellulose calcium, nitrocellulose In element, polyvinyl alcohol, polyvinyl butyral resin, polyvinyl formal acetal, polyvinyl acetate, polyvinylpyrrolidone one Plant or at least two mixtures for being constituted.
Wherein, the surfactant is made up of the one kind in lecithin, Span -85, Tween-80 or at least two Mixture；The dispersant be triammonium citrate, polymethyl acid amide, 1,4- dihydroxy sulfanilic acids in one kind or At least two mixtures for being constituted；The plasticizer is repefral, diethyl phthalate, O-phthalic A kind of or at least two mixtures for being constituted in dibutyl phthalate, dioctyl phthalate.
Wherein, the defoamer is organosiloxane, polyethers, polyethylene glycol, ethylene-acrylic acid copolymer, polyglycerol ester A kind of or at least two mixtures for being constituted in fat acid esters, dimethyl silicone polymer, organic silicon modified by polyether.
Wherein, the thixotropic agent is hexadecanol, polyamide wax, rilanit special, thixotropy alkyd resin, organobentonite Or a kind of or at least two mixtures for being constituted in aerosil.
A kind of preparation method of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, includes following processing step, Specially：
A, prepare microcrystalline glass powder：By SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, CaO be well mixed in three-dimensional material mixer, SiO in mixture2、Bi2O3、B2O3、ZnO、K2O、SrO2, in CaO the weight portion of seven kinds of materials be followed successively by 20% ~ 30%, 10% ~ 20%th, 10% ~ 20%, 10% ~ 20%, 10% ~ 20%, 5% ~ 10%, 5% ~ 10%, then at smelting furnace melting after being well mixed, smelting temperature is 1000 DEG C ~ 1200 DEG C, temperature retention time obtained glass melts for 3 ~ 6 hours, then glass melts is carried out into water quenching and obtains glass Glass, is finally medium to glass ball milling 4 ~ 6 hours with distilled water, that is, obtain the leadless crystallizing glass powder that particle size values are 1 ~ 3 μm；
B, prepare organic bonding phase：By organic solvent, macromolecule thickener, surfactant, plasticizer, dispersant, defoamer, Thixotropic agent dissolves to obtain organic bonding phase, and by adjusting the content of macromolecule thickener, so that organic in 80 DEG C of water-baths The viscosity of bonding phase is controlled in the range of 200 mPas ~ 300 mPas, wherein, organic solvent, high score in organic bonding phase Sub- thickener, surfactant, plasticizer, dispersant, defoamer, the weight portion of seven kinds of materials of thixotropic agent be followed successively by 30% ~ 60%, 20%~30%、1%~5%、1%~5%、1%~5%、1%~5%、1%~5%；
It is prepared by c, dielectric paste：By leadless crystallizing glass powder, rare earth oxide, organic bonding in container dispersed with stirring, and After be placed in three-roll grinder and grind repeatedly, to obtain dielectric paste of the range of viscosities as 40 ~ 60Pas, fineness less than 5 μm, Wherein, in dielectric paste leadless crystallizing glass powder, rare earth oxide, the weight portion of three kinds of materials of organic bonding phase be followed successively by 60% ~ 80%、1%~10%、19%~30%。
Beneficial effects of the present invention are：The invention discloses a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste And preparation method thereof, the preparation method is used to prepare aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, wherein, the present invention Aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste there is advantages below, specially：
1st, SiO is adopted2、Bi2O3、B2O3、ZnO、K2O、SrO2, the compound leadless crystallizing glass powder that formed of CaO, can significantly drop The smelting temperature of low material, makes dielectric layer in 450 DEG C ~ 550 DEG C sintering, it is to avoid lead after researching and developing, using and be discarded to environment, The injury that human body is caused, can solve high-power resistance or heating manufacturing urgent problem, meet European Union RoHS is instructed（2002/95/EC）Require；
2nd, by SiO2-Bi2O3-B2O3-ZnO-K2O-SrO2The thermal coefficient of expansion of-CaO microcrystalline glass in series, vitrification point, The regulation of softening temperature is allowed to mutually be combined the thermal coefficient of expansion and aluminium alloy of the dielectric layer for constituting with rare earth oxide, organic bonding Substrate is matched and with good binding ability, while firm network structure can be formed, makes composite microcrystallite glass insulate Dielectric material has good hardness and pliability, adapts to the requirement of aluminium alloy base plate thick film circuit work under bad environment；
3rd, dielectric paste of the invention be printed on the dielectric layer formed on aluminium alloy base plate and have that adhesive force is strong, breakdown strength is big, Insulaion resistance height and advantage that can be compatible with the thick film circuit resistance slurry of aluminium alloy base plate and electrode slurry, the preparation technology It is simple to operate, easily controllable, be advantageously implemented scale industrial production.
Specific embodiment
With reference to specific embodiment, the present invention will be described.
Embodiment 1
A kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, by weight percentage, including following components：
Leadless crystallizing glass powder 70%
Y2O3 5%
Organic bonding phase 25%；
The leadless crystallizing glass powder, by weight percentage, including following components：
SiO2 20%
Bi2O3 20%
B2O3 15%
ZnO 15%
K2O 15%
SrO2 10%
CaO 5%；
The organic bonding phase, by weight percentage, including following components：
Butyl carbitol 60%
Ethyl cellulose 25%
Tween-80 3%
Dibutyl phthalate 3%
Polymethyl acid amide 3%
Organic silicon modified by polyether 3%
Rilanit special 3%.
By above-mentioned material proportion, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment one have with Lower advantage, specially：
1st, SiO is adopted2、Bi2O3、B2O3、ZnO、K2O、SrO2, the compound leadless crystallizing glass powder that formed of CaO, can significantly drop The smelting temperature of low material, makes dielectric layer in 450 DEG C ~ 550 DEG C sintering, it is to avoid lead after researching and developing, using and be discarded to environment, The injury that human body is caused, can solve high-power resistance or heating manufacturing urgent problem, meet European Union RoHS is instructed（2002/95/EC）Require；
2nd, by SiO2-Bi2O3-B2O3-ZnO-K2O-SrO2The thermal coefficient of expansion of-CaO microcrystalline glass in series, vitrification point, The regulation of softening temperature is allowed to mutually be combined the thermal coefficient of expansion and aluminium alloy of the dielectric layer for constituting with rare earth oxide, organic bonding Substrate is matched and with good binding ability, while firm network structure can be formed, makes composite microcrystallite glass insulate Dielectric material has good hardness and pliability, adapts to the requirement of aluminium alloy base plate thick film circuit work under bad environment；
3rd, the dielectric paste of the present embodiment one is printed on the dielectric layer formed on aluminium alloy base plate and has that adhesive force is strong, breakdown strength Greatly, insulaion resistance it is high and can be compatible with the thick film circuit resistance slurry of aluminium alloy base plate and electrode slurry advantage, the preparation Technological operation is simple, easily controllable, be advantageously implemented scale industrial production.
Wherein, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment one can adopt following preparation sides Method is prepared from, specifically, a kind of preparation method of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, including following step Suddenly：
A, prepare leadless crystallizing glass powder：By SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, CaO mixes in three-dimensional material mixer Then at smelting furnace melting after even, smelting temperature is 1100 DEG C, and temperature retention time obtained glass melts for 4 hours, then melted in glass Liquid carries out water quenching and obtains glass, is finally medium to glass ball milling 4 hours with distilled water, that is, obtain particle size values for 1 ~ 3 μm Leadless crystallizing glass powder；
B, prepare organic bonding phase：By butyl carbitol, ethyl cellulose, Tween-80, dibutyl phthalate, poly- methyl Acrylic amine, organic silicon modified by polyether, rilanit special dissolve to obtain organic bonding phase, organic bonding phase in 80 DEG C of water-baths Viscosity be 240 ± 20 mPas；
C, prepare dielectric paste：By leadless crystallizing glass powder, rare earth oxide Y2O3, organic bonding stirs point in container Dissipate, be then placed in three-roll grinder and grind repeatedly, to obtain medium of the range of viscosities as 40 ± 10Pas, fineness less than 5 μm Slurry.
For the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment one, with silk screen in aluminium alloy base plate Upper printing film forming, 450 DEG C sintering after thickness of dielectric layers be 118 m, breakdown voltage（AC）>2000V, insulaion resistance（500V） 20M Ω, leakage current（250V）<2mA.
Embodiment 2
A kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, by weight percentage, including following components：
Leadless crystallizing glass powder 75%
La2O3 5%
Organic bonding phase 20%；
The leadless crystallizing glass powder, by weight percentage, including following components：
SiO2 20%
Bi2O3 10%
B2O3 20%
ZnO 15%
K2O 15%
SrO2 10%
CaO 10%；
The organic bonding phase, by weight percentage, including following components：
N,N-dimethylformamide 60%
Polyvinyl butyral resin 25%
Tween-80 3%
Dibutyl phthalate 3%
Polymethyl acid amide 3%
Organic silicon modified by polyether 3%
Rilanit special 3%.
By above-mentioned material proportion, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment two have with Lower advantage, specially：
1st, SiO is adopted2、Bi2O3、B2O3、ZnO、K2O、SrO2, the compound leadless crystallizing glass powder that formed of CaO, can significantly drop The smelting temperature of low material, makes dielectric layer in 450 DEG C ~ 550 DEG C sintering, it is to avoid lead after researching and developing, using and be discarded to environment, The injury that human body is caused, can solve high-power resistance or heating manufacturing urgent problem, meet European Union RoHS is instructed（2002/95/EC）Require；
2nd, by SiO2-Bi2O3-B2O3-ZnO-K2O-SrO2The thermal coefficient of expansion of-CaO microcrystalline glass in series, vitrification point, The regulation of softening temperature is allowed to mutually be combined the thermal coefficient of expansion and aluminium alloy of the dielectric layer for constituting with rare earth oxide, organic bonding Substrate is matched and with good binding ability, while firm network structure can be formed, makes composite microcrystallite glass insulate Dielectric material has good hardness and pliability, adapts to the requirement of aluminium alloy base plate thick film circuit work under bad environment；
3rd, the dielectric paste of the present embodiment two is printed on the dielectric layer formed on aluminium alloy base plate and has that adhesive force is strong, breakdown strength Greatly, insulaion resistance it is high and can be compatible with the thick film circuit resistance slurry of aluminium alloy base plate and electrode slurry advantage, the preparation Technological operation is simple, easily controllable, be advantageously implemented scale industrial production.
Wherein, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment two can adopt following preparation sides Method is prepared from, specifically, a kind of preparation method of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, including following step Suddenly：
A, prepare leadless crystallizing glass powder：By SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, CaO mixes in three-dimensional material mixer Then at smelting furnace melting after even, smelting temperature obtained glass melts for 1100 DEG C of temperature retention times for 3 hours, then by glass melts Carry out water quenching and obtain glass, be finally medium to glass ball milling 4 hours with distilled water, that is, obtain the nothing that particle size values are 1 ~ 3 μm Lead microcrystalline glass powder；
B, prepare organic bonding phase：By N,N-dimethylformamide, polyvinyl butyral resin, Tween-80, phthalic acid two Butyl ester, polymethyl acid amide, organic silicon modified by polyether, rilanit special dissolve to obtain organic bonding in 80 DEG C of water-baths Phase, the viscosity of organic bonding phase is 240 ± 20 mPas；
C, prepare dielectric paste：By leadless crystallizing glass powder, rare earth oxide La2O3, organic bonding stirs point in container Dissipate, be then placed in three-roll grinder and grind repeatedly, to obtain medium of the range of viscosities as 40 ± 10Pas, fineness less than 5 μm Slurry.
For the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment two, with silk screen in aluminium alloy base plate Upper printing film forming, 500 DEG C sintering after thickness of dielectric layers be 118 m, breakdown voltage（AC）>2000V, insulaion resistance（500V） 20M Ω, leakage current（250V）<2mA.
Embodiment 3
A kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, by weight percentage, including following components：
Leadless crystallizing glass powder 77%
Eu2O3 3%
Organic bonding phase 20%；
The leadless crystallizing glass powder, by weight percentage, including following components：
SiO2 25%
Bi2O3 15%
B2O3 10%
ZnO 15%,
K2O 15%
SrO2 10%
CaO 10%；
The organic bonding phase, by weight percentage, including following components：
Mixed dibasic acid ester 60%
Polyvinylpyrrolidone 25%
Tween-80 3%
Dibutyl phthalate 3%
Polymethyl acid amide 3%
Organic silicon modified by polyether 3%
Thixotropy alkyd resin 3%.
By above-mentioned material proportion, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment three have with Lower advantage, specially：
1st, SiO is adopted2、Bi2O3、B2O3、ZnO、K2O、SrO2, the compound leadless crystallizing glass powder that formed of CaO, can significantly drop The smelting temperature of low material, makes dielectric layer in 450 DEG C ~ 550 DEG C sintering, it is to avoid lead after researching and developing, using and be discarded to environment, The injury that human body is caused, can solve high-power resistance or heating manufacturing urgent problem, meet European Union RoHS is instructed（2002/95/EC）Require；
2nd, by SiO2-Bi2O3-B2O3-ZnO-K2O-SrO2The thermal coefficient of expansion of-CaO microcrystalline glass in series, vitrification point, The regulation of softening temperature is allowed to mutually be combined the thermal coefficient of expansion and aluminium alloy of the dielectric layer for constituting with rare earth oxide, organic bonding Substrate is matched and with good binding ability, while firm network structure can be formed, makes composite microcrystallite glass insulate Dielectric material has good hardness and pliability, adapts to the requirement of aluminium alloy base plate thick film circuit work under bad environment；
3rd, the dielectric paste of the present embodiment three is printed on the dielectric layer formed on aluminium alloy base plate and has that adhesive force is strong, breakdown strength Greatly, insulaion resistance it is high and can be compatible with the thick film circuit resistance slurry of aluminium alloy base plate and electrode slurry advantage, the preparation Technological operation is simple, easily controllable, be advantageously implemented scale industrial production.
Wherein, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment three can adopt following preparation sides Method is prepared from, specifically, a kind of preparation method of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, including following step Suddenly：
A, prepare leadless crystallizing glass powder：By SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, CaO mixes in three-dimensional material mixer Then at smelting furnace melting after even, smelting temperature is 1200 DEG C, and temperature retention time obtained glass melts for 3 hours, then melted in glass Liquid carries out water quenching and obtains glass, is finally medium to glass ball milling 4 hours with distilled water, that is, obtain particle size values for 1 ~ 3 μm Leadless crystallizing glass powder；
B, prepare organic bonding phase：By mixed dibasic acid ester, polyvinylpyrrolidone, Tween-80, dibutyl phthalate, Polymethyl acid amide, organic silicon modified by polyether, thixotropy alkyd resin dissolve to obtain organic bonding phase in 80 DEG C of water-baths, The viscosity of organic bonding phase is 240 ± 20 mPas；
C, prepare dielectric paste：By leadless crystallizing glass powder, rare earth oxide Eu2O3, organic bonding stirs point in container Dissipate, be then placed in three-roll grinder and grind repeatedly, to obtain medium of the range of viscosities as 40 ± 10Pas, fineness less than 5 μm Slurry.
For the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment three, with silk screen in aluminium alloy base plate Upper printing film forming, 550 DEG C sintering after thickness of dielectric layers be 118 m, breakdown voltage（AC）>2000V, insulaion resistance（500V） 20M Ω, leakage current（250V）<2mA.
Embodiment 4
A kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, by weight percentage, including following components：
Leadless crystallizing glass powder 65%
Sm2O3 5%
Organic bonding phase 30%；
The leadless crystallizing glass powder, by weight percentage, including following components：
SiO2 20%
Bi2O3 20%
B2O3 10%
ZnO 15%
K2O 15%
SrO2 10%
CaO 10%；
The organic bonding phase, by weight percentage, including following components：
Butyl carbitol acetate 60%
NC Nitroncellulose 25%
Lecithin 3%
Dibutyl phthalate 3%
Polymethyl acid amide 3%
Organic silicon modified by polyether 3%
Polyamide wax 3%.
By above-mentioned material proportion, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment four have with Lower advantage, specially：
1st, SiO is adopted2、Bi2O3、B2O3、ZnO、K2O、SrO2, the compound leadless crystallizing glass powder that formed of CaO, can significantly drop The smelting temperature of low material, makes dielectric layer in 450 DEG C ~ 550 DEG C sintering, it is to avoid lead after researching and developing, using and be discarded to environment, The injury that human body is caused, can solve high-power resistance or heating manufacturing urgent problem, meet European Union RoHS is instructed（2002/95/EC）Require；
2nd, by SiO2-Bi2O3-B2O3-ZnO-K2O-SrO2The thermal coefficient of expansion of-CaO microcrystalline glass in series, vitrification point, The regulation of softening temperature is allowed to mutually be combined the thermal coefficient of expansion and aluminium alloy of the dielectric layer for constituting with rare earth oxide, organic bonding Substrate is matched and with good binding ability, while firm network structure can be formed, makes composite microcrystallite glass insulate Dielectric material has good hardness and pliability, adapts to the requirement of aluminium alloy base plate thick film circuit work under bad environment；
3rd, the dielectric paste of the present embodiment four is printed on the dielectric layer formed on aluminium alloy base plate and has that adhesive force is strong, breakdown strength Greatly, insulaion resistance it is high and can be compatible with the thick film circuit resistance slurry of aluminium alloy base plate and electrode slurry advantage, the preparation Technological operation is simple, easily controllable, be advantageously implemented scale industrial production.
Wherein, the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment four can adopt following preparation sides Method is prepared from, specifically, a kind of preparation method of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, including following step Suddenly：
A, prepare leadless crystallizing glass powder：By SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, CaO mixes in three-dimensional material mixer Then at smelting furnace melting after even, smelting temperature is 1100 DEG C, and temperature retention time obtained glass melts for 3 hours, then melted in glass Liquid carries out water quenching and obtains glass, is finally medium to glass ball milling 4 hours with distilled water, that is, obtain particle size values for 1 ~ 3 μm Leadless crystallizing glass powder；
B, prepare organic bonding phase：By terpinol, NC Nitroncellulose, lecithin, dibutyl phthalate, polymethylacrylic acid Amine, organic silicon modified by polyether, polyamide wax dissolve to obtain organic bonding phase in 80 DEG C of water-baths, and the viscosity of organic bonding phase is 240±20 mPa·s；
C, prepare dielectric paste：By leadless crystallizing glass powder, rare earth oxide Sm2O3, organic bonding stirs point in container Dissipate, be then placed in three-roll grinder and grind repeatedly, to obtain medium of the range of viscosities as 45 ± 10Pas, fineness less than 5 μm Slurry.
For the aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste of the present embodiment four, with silk screen in aluminium alloy base plate Upper printing film forming, 530 DEG C sintering after thickness of dielectric layers be 105 m, breakdown voltage（AC）>2000V, insulaion resistance（500V） 20M Ω, leakage current（250V）<2mA.
Above content is only presently preferred embodiments of the present invention, for one of ordinary skill in the art, according to the present invention's Thought, will change in specific embodiments and applications, and this specification content should not be construed as to the present invention Restriction.

Claims (9)

1. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, it is characterised in that include the thing of following weight portion Material, specially：
Leadless crystallizing glass powder 60% ~ 80%
Rare earth oxide 1% ~ 10%
Organic bonding phase 19% ~ 30%；
Wherein, leadless crystallizing glass powder is by SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, seven kinds of materials of CaO composition, unleaded crystallite SiO in glass dust2、Bi2O3、B2O3、ZnO、K2O、SrO2, seven kinds of materials of CaO weight portion be followed successively by 20% ~ 30%, 10% ~ 20%, 10%~20%、10%~20%、10%~20%、5%~10%、5%~10%；
Organic bonding is mutually organic solvent, macromolecule thickener, surfactant, plasticizer, dispersant, defoamer, thixotropic agent The mixture that seven kinds of materials are constituted, organic solvent in organic bonding phase, macromolecule thickener, surfactant, plasticizer, point Powder, defoamer, the weight portion of eight kinds of materials of thixotropic agent be followed successively by 30% ~ 60%, 20% ~ 30%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%, 1% ~ 5%、1%~5%。
2. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute The particle size values for stating leadless crystallizing glass powder are 1 ~ 3 μm, and softening point is 350 ~ 450 DEG C, and average coefficient of linear expansion is 18 ~ 25 × 10-6/ ℃。
3. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute Rare earth oxide is stated for La2O3、Sc2O3、Y2O3、CeO2、Sm2O3、Gd2O3、Nd2O3、Pr2O3、Eu2O3In one kind, rare-earth oxidation The particle size values of thing are 1 ~ 3 μm.
4. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute State organic solvent for turpentine oil, terpinol, hexadecanol, butyl carbitol, butyl carbitol acetate, diethylene glycol monomethyl ether, Dibutyl ethylene glycol ether, ethylene glycol ether acetate, ATBC, tributyl phosphate, GBL, mixed dibasic acid One kind in ester, 1-METHYLPYRROLIDONE, DMF, DMA, dimethyl sulfoxide or at least Two kinds of mixtures for being constituted.
5. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute Macromolecule thickener is stated for ethyl cellulose, hydroxyethyl cellulose, carboxymethylcellulose calcium, NC Nitroncellulose, polyvinyl alcohol, poly- second One kind or at least two institutes in enol butyral, polyvinyl formal acetal, polyvinyl acetate, polyvinylpyrrolidone The mixture of composition.
6. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute A kind of or at least two mixtures for constituting during surfactant is stated by lecithin, Span -85, Tween-80；Described point Powder by triammonium citrate, polymethyl acid amide, 1,4- dihydroxy sulfanilic acids in it is a kind of or at least two constitute Mixture；The plasticizer is repefral, diethyl phthalate, dibutyl phthalate, adjacent benzene two A kind of or at least two mixtures for being constituted in formic acid dioctyl ester.
7. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute Defoamer is stated for organosiloxane, polyethers, polyethylene glycol, ethylene-acrylic acid copolymer, polyglyceryl fatty acid ester, poly dimethyl A kind of or at least two mixtures for being constituted in siloxanes, organic silicon modified by polyether.
8. a kind of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste according to claim 1, it is characterised in that：Institute Thixotropic agent is stated for hexadecanol, polyamide wax, rilanit special, thixotropy alkyd resin, organobentonite or aerosil In a kind of or at least two mixtures for being constituted.
9. a kind of preparation method of aluminium alloy base plate thick film circuit intermediate sintering temperature dielectric paste, it is characterised in that include following Processing step, specially：
A, prepare microcrystalline glass powder：By SiO2、Bi2O3、B2O3、ZnO、K2O、SrO2, CaO be well mixed in three-dimensional material mixer, mix SiO in compound2、Bi2O3、B2O3、ZnO、K2O、SrO2, in CaO the weight portion of seven kinds of materials be followed successively by 20% ~ 30%, 10% ~ 20%, 10% ~ 20%, 10% ~ 20%, 10% ~ 20%, 5% ~ 10%, 5% ~ 10%, then at smelting furnace melting after being well mixed, smelting temperature is 1000 DEG C ~ 1200 DEG C, temperature retention time obtained glass melts for 3 ~ 6 hours, then glass melts is carried out into water quenching and obtains glass, finally It is medium to glass ball milling 4 ~ 6 hours with distilled water, that is, obtains the leadless crystallizing glass powder that particle size values are 1 ~ 3 μm；
B, prepare organic bonding phase：By organic solvent, macromolecule thickener, surfactant, plasticizer, dispersant, defoamer, Thixotropic agent dissolves to obtain organic bonding phase, and by adjusting the content of macromolecule thickener, so that organic in 80 DEG C of water-baths The viscosity of bonding phase is controlled in the range of 200 mPas ~ 300 mPas, wherein, organic solvent, high score in organic bonding phase Sub- thickener, surfactant, plasticizer, dispersant, defoamer, the weight portion of seven kinds of materials of thixotropic agent be followed successively by 30% ~ 60%, 20%~30%、1%~5%、1%~5%、1%~5%、1%~5%、1%~5%；
It is prepared by c, dielectric paste：By leadless crystallizing glass powder, rare earth oxide, organic bonding in container dispersed with stirring, and After be placed in three-roll grinder and grind repeatedly, to obtain dielectric paste of the range of viscosities as 40 ~ 60Pas, fineness less than 5 μm, Wherein, in dielectric paste leadless crystallizing glass powder, rare earth oxide, the weight portion of three kinds of materials of organic bonding phase be followed successively by 60% ~ 80%、1%~10%、19%~30%。
CN201610853299.4A 2016-09-27 2016-09-27 Aluminum alloy substrate thick film circuit intermediate-temperature sintering dielectric paste and preparation method thereof Pending CN106571172A (en)

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